WO2018025813A1 - Oil concentration measuring device and oil concentration measuring method - Google Patents

Oil concentration measuring device and oil concentration measuring method Download PDF

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Publication number
WO2018025813A1
WO2018025813A1 PCT/JP2017/027732 JP2017027732W WO2018025813A1 WO 2018025813 A1 WO2018025813 A1 WO 2018025813A1 JP 2017027732 W JP2017027732 W JP 2017027732W WO 2018025813 A1 WO2018025813 A1 WO 2018025813A1
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WIPO (PCT)
Prior art keywords
oil
concentration
cleaning
light
wavelength
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PCT/JP2017/027732
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French (fr)
Japanese (ja)
Inventor
和久 小笠原
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アクトファイブ株式会社
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Application filed by アクトファイブ株式会社 filed Critical アクトファイブ株式会社
Priority to JP2018531888A priority Critical patent/JP7153923B2/en
Priority to CN201780048765.4A priority patent/CN109564158A/en
Publication of WO2018025813A1 publication Critical patent/WO2018025813A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

Definitions

  • the present invention relates to an apparatus and a method for measuring the concentration of oil in a cleaning liquid.
  • This oil concentration measuring device and oil concentration measuring method is contained in the cleaning liquid used in industrial cleaning machines that remove oils such as cutting oil, press / punching oil, machine oil, grease, and flux adhering to the workpiece. It is suitably used for measuring the concentration of oil.
  • the cleaning liquid used in industrial cleaning machines is mainly hydrocarbon cleaning liquid. Since the hydrocarbon-based cleaning liquid does not contain an ozone-depleting substance or chlorine, it has a feature that it has little influence on the environment and the human body. In addition, by utilizing the fact that hydrocarbons have a lower boiling point than the above oil component, the hydrocarbon cleaning liquid is a hydrocarbon after storing the used hydrocarbon cleaning liquid in the distillation tank. It is also possible to recycle by heating to a temperature higher than the boiling point of the oil and lower than the boiling point of the oil component.
  • the hydrocarbon-based cleaning liquid further has a feature that clean steam generated during the distillation regeneration treatment can be used for cleaning and drying of the workpiece (hereinafter referred to as “steam cleaning / drying”).
  • the work In steam cleaning / drying, the work is stored in a steam cleaning / drying cleaning tank, the surface of the work is cleaned with the steam by introducing the steam into the tank, and then the inside of the tank is rapidly depressurized. By rapidly lowering the boiling point of the cleaning agent, the cleaning agent adhering to the work surface is bumped and vaporized, and the work is dried.
  • a workpiece In an actual industrial cleaning machine, a workpiece is stored in a liquid cleaning tank in which a hydrocarbon-based cleaning liquid is stored and liquid cleaning is performed, and then steam cleaning and drying are performed for finishing.
  • the oil removed by the distillation gradually accumulates in the distillation tank, and the oil is mixed into the vapor of the hydrocarbon-based cleaning liquid after the distillation regeneration (cleaning liquid after the regeneration). If it does so, the oil component in vapor
  • the predetermined concentration differs depending on the component of the oil component, but it is desirable to set it to 50 to 100 ppm or less in order to prevent the cleaning ability from being lowered regardless of the component.
  • the remaining liquid in the distillation tank containing oil is removed when the number of times the workpiece has been cleaned reaches a predetermined number determined by empirical rules, but if the concentration of oil in the cleaning liquid after regeneration is measured, It is expected that the residual liquid can be removed at an appropriate timing.
  • Patent Document 1 In order to measure the oil concentration of the cleaning liquid, for example, the method described in Patent Document 1 can be used.
  • the absorbance is measured using ultraviolet light having a predetermined measurement wavelength determined for each component of the oil contained in the cleaning liquid, and a calibration curve of the oil concentration and the absorbance prepared in advance is prepared. Is used to determine the concentration of oil dissolved in the cleaning liquid.
  • the measurement wavelength for each oil component is, for example, 259 nm for commercially available press oil, 234 nm for commercially available cutting oil, and 250 nm for commercially available flux.
  • the problem to be solved by the present invention is to provide an apparatus and a method for measuring the oil concentration in a cleaning liquid that do not require the use of expensive spectroscopic elements, detection elements, and control equipment.
  • the oil concentration measuring device in the cleaning liquid according to the present invention made to solve the above problems, a) a light irradiation unit for irradiating the measurement target liquid with irradiation light having a measurement wavelength which is a predetermined wavelength between 280 and 300 nm; b) a transmitted light detector that measures the intensity of transmitted light through which the irradiation light has transmitted through the measurement target liquid; c) Based on the intensity of the transmitted light measured by the transmitted light detection unit, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and the relationship between the absorbance value and the concentration of oil and absorbance at the measurement wavelength is calculated. And an oil concentration determination unit that obtains the concentration of the oil in the measurement target liquid based on a calibration curve that is shown.
  • cleaning liquids such as hydrocarbon cleaning liquids, which are currently mainstream as cleaning liquids for industrial cleaning machines, and other glycol ether cleaning liquids, have multiple (double and triple) bonding of carbon atoms. It consists of molecules that do not have Molecules that do not have such multiple bonds of carbon atoms will absorb light at a wavelength of less than 280 nm, while light absorption will hardly occur at wavelengths of 280 nm or longer.
  • most of oils such as cutting oil, press / punching oil, machine oil, grease, and flux that adhere to the workpiece to be cleaned and are mixed into the cleaning liquid by cleaning contain molecules having multiple bonds of carbon atoms.
  • Molecules having such multiple bonds of carbon atoms have a broad range of wavelengths at which the absorbance peaks depending on the type, but the absorbance is 0 within the wavelength range of 280 to 300 nm regardless of the type of oil. It has a constant value. Furthermore, when the wavelength exceeds 300 nm, it becomes difficult to detect an oil component having a low concentration of about 50 ppm.
  • the intensity of transmitted light is measured at a measurement wavelength which is a predetermined one wavelength between 280 and 300 nm, and the absorbance at the measurement wavelength is calculated based on the intensity, whereby the measurement target liquid (cleaning liquid, measurement).
  • concentration of the oil can be determined based on a calibration curve indicating the relationship between the oil content to be measured and the absorbance at the measurement wavelength while suppressing the influence of light absorption by the target cleaning solution.
  • the oil concentration measuring apparatus since only one predetermined wavelength is used as the measurement wavelength, it is not necessary to use a spectroscopic element or a detection element for each wavelength.
  • the amount of data to be processed simultaneously is smaller than in the case of using a plurality of wavelengths, it is not necessary to use an expensive control device.
  • the oil concentration measuring device can be controlled using a control device (programmable logic controller) of an industrial washing machine without providing a dedicated control device for the oil concentration measuring device according to the present invention. For these reasons, the oil concentration measuring device according to the present invention can reduce the cost.
  • the oil concentration measuring apparatus can be suitably used for measuring oil components having a low concentration of 50 to 2000 ppm.
  • the oil-concentration measurement device according to the present invention is used for the above-described steam cleaning / drying that requires the ability to detect a low-concentration oil content of 50 ppm. It can be suitably used for measuring the oil concentration in the post-regeneration cleaning liquid.
  • the target of oil content measurement by the oil concentration measuring device according to the present invention is not limited to the cleaning liquid after regeneration. It can also be used for obtaining (when the time change of the oil concentration becomes equal to or less than a predetermined value is set as the end timing).
  • the oil concentration measuring device further includes: A second light irradiation unit that irradiates the measurement target liquid with a second irradiation light having a second measurement wavelength that is a predetermined one wavelength between 320 and 340 nm; A second transmitted light detector that measures the intensity of the second transmitted light through which the second irradiation light has passed through the measurement target liquid; Based on the intensity of the second transmitted light measured by the second transmitted light detection unit, the absorbance at the second measurement wavelength of the measurement target liquid is calculated, and the value of the absorbance and the oil content at the second measurement wavelength are calculated.
  • the second having the second measurement wavelength which is a predetermined one wavelength between 320 and 340 nm.
  • the detector for detecting the transmitted light does not need to recognize the wavelength.
  • This detector can be used.
  • a photodiode can be suitably used for such a detector.
  • the method for measuring the oil concentration in the cleaning liquid according to the present invention is as follows. Irradiate the measurement target liquid with irradiation light having a predetermined measurement wavelength of 280 to 300 nm, Measure the intensity of transmitted light through which the irradiation light has passed through the measurement target liquid, Based on the intensity of the transmitted light, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and based on the absorbance value and a calibration curve indicating the relationship between the oil content and the absorbance at the measurement wavelength, It is characterized by determining the concentration of oil.
  • the schematic block diagram which shows the industrial washing machine which has one Embodiment of the oil concentration measuring apparatus which concerns on this invention as a component.
  • the figure which shows the measured value of the spectrum of the transmitted light amount in four types of washing
  • the functional block diagram which shows the function of the control part in the oil concentration measuring apparatus of this embodiment.
  • the graph which shows the result of having measured the transmitted light amount of the washing
  • required the light absorbency from the transmitted light amount shown in FIG. 6 is a graph showing a calibration curve for each oil component created based on the absorbance shown in FIG. 5.
  • FIG. 1 shows a schematic configuration of an industrial washing machine 1 having an oil concentration measuring device 10 of this embodiment as a component.
  • the industrial cleaning machine 1 is a device for removing oil adhering to a workpiece.
  • the first cleaning tank 11, the second cleaning tank 12, the steam cleaning / drying tank 13, and the temporary It has a storage tank 14, a distillation tank 15, a heat exchanger 16, an ejector 17, a post-regeneration cleaning liquid storage tank 18, and a sample cell cleaning liquid tank 19.
  • a thick solid line indicates a liquid flow path
  • a thick broken line indicates a gas flow path
  • a thin straight broken line indicates an electric signal path.
  • the first cleaning tank 11 and the second cleaning tank 12 are provided with an ultrasonic vibrator that applies ultrasonic vibration to the cleaning liquid stored in the tank. Moreover, in order to make it easy to produce cavitation by an ultrasonic wave, the inside of the 1st washing tank 11 and the 2nd washing tank 12 is pressure-reduced with a vacuum pump, and deaeration of a washing
  • the oil content of the cleaning liquid in the second cleaning tank 12 is smaller than the cleaning liquid in the first cleaning tank 11, the work is first cleaned in the first cleaning tank 11. Then, by cleaning the workpiece in the second cleaning tank 12, it is possible to minimize the oil in the cleaning liquid from reattaching to the workpiece.
  • the steam cleaning / drying tank 13 is a tank for performing steam cleaning and drying on the workpiece cleaned in the second cleaning tank 12.
  • the steam used for steam cleaning / drying is supplied from the distillation tank 15 as described later.
  • the cleaning liquid from which the steam in the steam cleaning / drying tank 13 and the material remaining on the surface of the work are removed is returned to the second cleaning tank 12. Further, the gas generated by the decompression of the first cleaning tank 11 and the second cleaning tank 12 and the evaporation of the cleaning liquid is collected in the temporary storage tank 14.
  • the distillation tank 15 is provided with a float valve 151, and when the liquid in the distillation tank 15 becomes a predetermined amount or less by distillation, the cleaning liquid is introduced from the temporary storage tank 14 into the distillation tank 15.
  • the distillation tank 15 is heated by a heater (not shown) and depressurized by an ejector 17. As a result, the cleaning liquid evaporates leaving the oil as a liquid.
  • a part of the generated steam is supplied to the steam cleaning / drying tank 13 as described above, and the rest is condensed in the heat exchanger 16 and then stored in the cleaning liquid storage tank 18 after regeneration.
  • the post-regeneration cleaning liquid from which oil has been removed by the distillation tank 15 flows from the post-regeneration cleaning liquid storage tank 18 into the second cleaning tank 12.
  • the first cleaning tank 11 and the second cleaning tank 12 are connected by a second overflow pipe 122.
  • the second overflow pipe 122 has a higher connection position with the second cleaning tank 12 than a connection position with the first cleaning tank 11, and the cleaning liquid in the second cleaning tank 12 flows due to the inflow of the cleaning liquid after regeneration.
  • the cleaning liquid in the second cleaning tank 12 has a smaller oil content than the cleaning liquid in the first cleaning tank 11.
  • first cleaning tank 11 and the temporary storage tank 14 are connected by a first overflow pipe 112, and the liquid level of the cleaning liquid in the first cleaning tank 11 is caused by the inflow of the cleaning liquid from the second cleaning tank 12. If it becomes higher than the connection position of the pipe
  • the 1st washing tank 11 has the 1st circulation filtration system 111 which takes out cleaning fluid from a tank, and returns it in a tank through a filter.
  • a similar second circulation filtration system 121 is also provided in the second cleaning tank 12. These circulating filtration systems remove particles having a particle size of about 10 ⁇ m or more, and cannot remove oil.
  • the oil concentration measuring apparatus 10 includes a flow path 101 connected to the first cleaning tank 11, the second cleaning tank 12, and the post-regeneration cleaning liquid storage tank 18, and a liquid feed pump 102 provided in the flow path 101, as will be described later. And a sample cell 103 provided downstream of the liquid feed pump 102 in the flow channel 101, a reference cell 1031 for reference measurement, a light irradiation unit 104, a transmitted light detection unit 105, and control of the entire apparatus. And a control unit 106 that performs data processing to be described later.
  • the inflow portion 1011 of the flow path 101 is supplied to the first cleaning tank 11 via the first relay pipe 113, to the second cleaning tank 12 via the second relay pipe 123, and after-regeneration cleaning liquid via the third relay pipe 183.
  • Each is connected to the storage tank 18.
  • the first relay pipe 113 is provided with a first relay on-off valve 11V
  • the second relay pipe 123 is provided with a second relay on-off valve 12V
  • the third relay pipe 183 is provided with a third relay on-off valve 18V. ing.
  • the outflow part of the channel 101 is connected to the temporary storage tank 14. Therefore, the cleaning liquid used for the measurement in the oil concentration measuring device 10 is distilled by the distillation tank 15 through the temporary storage tank 14, and finally returned to the second cleaning tank 12 in a state where the oil is removed. In addition, you may make it return the washing
  • Both the sample cell 103 and the reference cell 1031 are quartz cells that absorb less ultraviolet light.
  • the sample cell 103 is connected to the channel 101 during normal measurement, and the reference cell 1031 is connected when measuring reference data.
  • the reference cell 1031 is filled with a cleaning liquid that does not contain oil, and the reference data is measured after interrupting the measurement of the oil concentration at predetermined time intervals under the control of the control unit 106.
  • the light irradiation unit 104 irradiates the cleaning liquid (measurement target liquid) in the sample cell 103 with a predetermined measurement wavelength between 280 and 300 nm, and emits the measurement wavelength. Consists of. In this embodiment, the measurement wavelength is 290 nm.
  • FIG. 2 shows measured values of the spectrum of transmitted light in the four types of cleaning liquids 1 to 4 composed of molecules having no multiple bonds of carbon atoms.
  • cleaning solutions 1 to 3 are all saturated aliphatic hydrocarbon cleaning solutions, and cleaning solution 4 is a glycol ether cleaning solution.
  • FIG. 2 also shows the spectrum of incident light. All of the four types of cleaning liquids have a transmitted light amount that is significantly smaller than the amount of incident light at a wavelength of less than 280 nm, and ultraviolet light is absorbed by the cleaning liquid.
  • the wavelength is 280 nm or more
  • the difference between the transmitted light amount and the incident light is small, and the ultraviolet rays are hardly absorbed by the cleaning liquid. Therefore, if the measurement is performed at a measurement wavelength of 280 nm, the concentration of the oil can be measured while suppressing the influence of light absorption by the cleaning liquid.
  • the measurement wavelength exceeds 300 nm, as shown in FIG. 5 to be described later, the absorbance value due to the oil component at a low concentration (100 ppm in the example shown in FIG. 5 and further 50 ppm) becomes too small. I can't. Therefore, by setting one wavelength between 280 and 300 nm as the measurement wavelength, it is possible to measure the oil concentration even at a low concentration of about 50 ppm while suppressing the influence of light absorption by the cleaning liquid.
  • the transmitted light detection unit 105 detects the intensity of transmitted light having the measurement wavelength that has passed through the cleaning liquid in the sample cell 103, and includes a photodiode and a signal conversion unit.
  • the photodiode detects the light of the measurement wavelength and outputs the intensity as an analog signal.
  • the signal converter converts the analog signal output from the photodiode into a digital signal.
  • the control unit 106 has the functions shown in the functional block diagram of FIG.
  • a programmable logic controller or a personal computer can be used, and a control device of an industrial cleaning machine may be applied as it is, or a control device of the oil concentration measuring device 10 may be provided.
  • the control unit 106 includes an oil concentration determination unit 1061, a reference data recording unit 1062, a calibration curve recording unit 1063, a condition input unit 1064, and a measurement control unit 1065.
  • the oil concentration determination unit 1061 includes an absorbance calculation unit 1061A, a calibration curve selection unit 1061B, and a calibration curve application unit 1061C. Details of the oil concentration determination unit 1061 will be described later together with the operation of the oil concentration measuring apparatus 10 of the present embodiment.
  • the reference data recording unit 1062 records transmitted light amount data (reference data) at the measurement wavelength, which is measured in advance for a cleaning agent that does not contain oil.
  • the calibration curve recording unit 1063 includes, for each oil component that can be used for processing the workpiece, the concentration and absorbance of the oil component at the measurement wavelength created based on data measured in advance using a sample having a known oil component concentration. A calibration curve showing the relationship is recorded. In addition, when components are close to each other between a plurality of processing oils having different manufacturers and model numbers, a common calibration curve may be used for the plurality of processing oils.
  • the condition input unit 1064 is used by the measurer to input measurement conditions described later using an input device such as a touch panel.
  • the measurement control unit 1065 controls the start and end of light irradiation from the light source in the light irradiation unit 104 and the start and end of the processing of each unit.
  • the sample cell cleaning liquid tank 19 is a tank in which a cleaning liquid for cleaning the sample cell 103 (the same as the cleaning liquid that is the target of oil concentration measurement) is stored.
  • measurement is started when the measurer inputs a predetermined measurement condition in the condition input unit 1064 and then inputs a measurement start instruction.
  • the measurement condition input here is information (for example, manufacturer and model number of the processing oil) for specifying the processing oil attached to the workpiece to be cleaned using the cleaning liquid to be measured.
  • the cleaning tank storing the cleaning liquid to be measured or the relay valve corresponding to the storage tank is opened.
  • the third relay open / close valve 18V provided in the third relay pipe 183 connected to the post-regeneration cleaning liquid storage tank 18 is opened.
  • the post-regeneration cleaning liquid to be measured is introduced into the sample cell 103 through the channel 101. If the cleaning liquid to be measured is the cleaning liquid in the first cleaning tank 11, the first relay on / off valve 11V is opened, and if the cleaning liquid in the second cleaning tank 12 is to be opened, the second relay on / off valve 12V is opened.
  • the light irradiation unit 104 irradiates the cleaning liquid in the sample cell 103 with light having the measurement wavelength (290 nm).
  • the transmitted light detection unit 105 measures the intensity I of the transmitted light amount that has passed through the cleaning liquid, converts it into a digital signal, and outputs it.
  • control unit 106 inputs a digital signal indicating the intensity I of the transmitted light amount output from the transmitted light detection unit 105 and transmits the transmitted light amount at the measurement wavelength of the cleaning liquid not containing oil from the reference data recording unit 1062.
  • Reference data I 0 is acquired.
  • the calibration curve selection unit 1061B of the control unit 106 generates a calibration curve corresponding to the specified processing oil based on the information for specifying the processing oil input by the condition input unit 1064. Get from. Then, the calibration curve application unit 1061C applies the absorbance A of the cleaning liquid to be measured obtained by the absorbance calculation unit 1061A to the calibration curve selected by the calibration curve selection unit 1061B, and obtains the concentration of the processing oil.
  • the concentration of the processing oil is repeatedly obtained by repeatedly introducing the cleaning liquid after regeneration to the sample cell 103 into the sample cell 103 and repeatedly performing the light irradiation by the light irradiation unit 104 and the measurement of the intensity I of the transmitted light amount.
  • concentration of the processing oil exceeds a predetermined value
  • the residual liquid remaining in the distillation tank 15 is processed.
  • the treatment of the residual liquid is performed by separating the cleaning liquid and the processing oil in the residual liquid by boiling the residual liquid, thereby discarding the processing oil remaining in the distillation tank 15.
  • the concentration of the processing oil in the cleaning liquid is repeatedly obtained by the same method as described above during the cleaning of the workpiece.
  • the measurement result can be used to determine the timing of completion of cleaning, that is, the cleaning of the workpiece is terminated when the change with time of the concentration becomes a predetermined value or less.
  • the amount of transmitted light obtained by the measurement is shown in FIG. 4 for each oil contained in the cleaning liquid. Moreover, the result of having calculated
  • a calibration curve showing the relationship between the absorbance and the concentration was prepared for each oil content.
  • the prepared calibration curve is shown in FIG.
  • data with a concentration of 10,000 ppm is not used because it deviates from the straight line in the calibration curve.
  • the concentration is 2000 ppm or less, the calibration curve can be shown as a straight line. Therefore, at a concentration of at least 2000 ppm, the oil concentration can be measured by the oil concentration measuring apparatus and method of this embodiment.
  • the oil concentration of the regenerated cleaning liquid that is distilled and regenerated in the distillation tank 15 is measured and managed continuously by an industrial cleaning machine. Most important to do while driving. According to the present invention, it is possible to measure and manage the oil concentration during continuous operation of such an industrial washer.
  • the light irradiation unit 104 irradiates the cleaning liquid with light having a measurement wavelength between 280 and 300 nm (290 nm in the above example).
  • the cleaning liquid may be irradiated with a second measurement wavelength that is a predetermined wavelength of 340 nm.
  • Such two different wavelengths of light are preferably generated using two light sources that emit monochromatic light and have different wavelengths of monochromatic light.
  • the transmitted light detection unit 105 can measure the intensities of both the light having the measurement wavelength and the light having the second measurement wavelength, only one light can be detected in common. I just need it. Or you may use the transmitted light detection part which changes for every wavelength.
  • the measurement wavelength 290 nm
  • a calibration curve showing the relationship between absorbance and concentration can be created for each oil component based on the absorbance data in FIG.
  • the calibration curve shown in Fig. 6 (d) has a slightly larger difference between the point where the absorbance was obtained and the calibration curve than the calibration curves (a) to (c).
  • the accuracy can be increased by obtaining the oil concentration.

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Abstract

Provided is an oil concentration measuring device for measuring the concentration of oil in a cleaning liquid, with which it is not necessary to use a costly spectroscopic element or detecting element, for example. An oil concentration measuring device 10 is provided with: a light radiating unit 104 which radiates radiating light having a measuring wavelength, which is one prescribed wavelength between 280 and 300 nm, onto a liquid to be measured (cleaning liquid); a transmitted light detecting unit 105 which measures the intensity of transmitted light resulting from the radiating light that has been transmitted through the liquid to be measured; and an oil concentration determining unit 1061 which calculates a light absorbency, at the measuring wavelength, of the liquid to be measured, on the basis of the intensity of the transmitted light measured by the transmitted light detecting unit 105, and obtains the concentration of oil in the liquid to be measured, on the basis of the value of the light absorbency, and a calibration curve indicating a relationship between the concentration of the oil and the light absorbency at the measuring wavelength. By using one wavelength between 280 and 300 nm at which molecules that do not have multiple carbon element bonds, included in hydrocarbon based cleaning liquids, which are mainstream industrial cleaning liquids, absorb almost no light, and with which it is possible to detect oil with a low concentration of approximately 50 ppm, a costly spectroscopic element or detecting element, for example, becomes unnecessary.

Description

油分濃度計測装置及び油分濃度計測方法Oil concentration measuring apparatus and oil concentration measuring method
 本発明は、洗浄液中の油分の濃度を計測する装置及び方法に関する。この油分濃度計測装置及び油分濃度計測方法は、ワークに付着した切削油、プレス・打抜き油、機械油、グリース、フラックス等の油分を除去する工業用洗浄機において、使用中の洗浄液等に含有される油分の濃度を計測するために好適に用いられるものである。 The present invention relates to an apparatus and a method for measuring the concentration of oil in a cleaning liquid. This oil concentration measuring device and oil concentration measuring method is contained in the cleaning liquid used in industrial cleaning machines that remove oils such as cutting oil, press / punching oil, machine oil, grease, and flux adhering to the workpiece. It is suitably used for measuring the concentration of oil.
 工業用洗浄機において使用される洗浄液は、炭化水素系洗浄液が主流となっている。炭化水素系洗浄液は、オゾン層破壊物質や塩素を含有しないため、環境や人体に与える影響が少ないという特長を有する。また、上記油分の成分よりも炭化水素の方が沸点が低いことを利用して、炭化水素系洗浄液は、使用後の油分を含有する炭化水素系洗浄液を蒸留槽内に貯留したうえで炭化水素の沸点よりも高く油分の沸点よりも低い温度に加熱することにより、蒸留再生することができるという特長も有する。炭化水素系洗浄液はさらに、この蒸留再生処理時に発生する清浄な蒸気をワークの洗浄及び乾燥(以下、「蒸気洗浄・乾燥」とする)に利用することができる、という特長も有する。蒸気洗浄・乾燥では、蒸気洗浄・乾燥用洗浄槽にワークを収容し、該槽に該蒸気を導入することによりワークの表面を該蒸気で洗浄した後、該槽内を急速に減圧することで洗浄剤の沸点を急激に低下させることにより、ワーク表面に付着していた洗浄剤を突沸・気化させ、該ワークを乾燥させる。実際の工業用洗浄機では、炭化水素系洗浄液が貯留された液体洗浄槽にワークを収容して液体洗浄を行った後、仕上げに蒸気洗浄・乾燥が行われる。 The cleaning liquid used in industrial cleaning machines is mainly hydrocarbon cleaning liquid. Since the hydrocarbon-based cleaning liquid does not contain an ozone-depleting substance or chlorine, it has a feature that it has little influence on the environment and the human body. In addition, by utilizing the fact that hydrocarbons have a lower boiling point than the above oil component, the hydrocarbon cleaning liquid is a hydrocarbon after storing the used hydrocarbon cleaning liquid in the distillation tank. It is also possible to recycle by heating to a temperature higher than the boiling point of the oil and lower than the boiling point of the oil component. The hydrocarbon-based cleaning liquid further has a feature that clean steam generated during the distillation regeneration treatment can be used for cleaning and drying of the workpiece (hereinafter referred to as “steam cleaning / drying”). In steam cleaning / drying, the work is stored in a steam cleaning / drying cleaning tank, the surface of the work is cleaned with the steam by introducing the steam into the tank, and then the inside of the tank is rapidly depressurized. By rapidly lowering the boiling point of the cleaning agent, the cleaning agent adhering to the work surface is bumped and vaporized, and the work is dried. In an actual industrial cleaning machine, a workpiece is stored in a liquid cleaning tank in which a hydrocarbon-based cleaning liquid is stored and liquid cleaning is performed, and then steam cleaning and drying are performed for finishing.
 工業用洗浄機を連続運転すると、蒸留により除去された油分が徐々に蒸留槽内に蓄積してゆき、蒸留再生後の炭化水素系洗浄液(再生後洗浄液)の蒸気に油分が混入してしまう。そうすると、蒸気洗浄・乾燥の際に蒸気中の油分がワークの表面に付着してしまい、洗浄の能力が低下してしまう。このような洗浄能力の低下を防止するためには、再生後洗浄液の油分濃度を所定濃度以下に抑える必要がある。当該所定濃度は油分の成分により相違するが、成分に依らずに洗浄能力の低下を防止するには50~100ppm以下とすることが望ましい。従来は、ワークの洗浄回数が経験則で定めた所定数に達したときに油分を含む蒸留槽内の残液を除去しているが、再生後洗浄液中の油分の濃度を測定すれば、より適切なタイミングで該残液の除去を行うことができることが期待される。 When the industrial cleaning machine is continuously operated, the oil removed by the distillation gradually accumulates in the distillation tank, and the oil is mixed into the vapor of the hydrocarbon-based cleaning liquid after the distillation regeneration (cleaning liquid after the regeneration). If it does so, the oil component in vapor | steam will adhere to the surface of a workpiece | work at the time of vapor cleaning and drying, and the capability of washing | cleaning will fall. In order to prevent such a decrease in cleaning ability, it is necessary to keep the oil concentration of the cleaning liquid after regeneration below a predetermined concentration. The predetermined concentration differs depending on the component of the oil component, but it is desirable to set it to 50 to 100 ppm or less in order to prevent the cleaning ability from being lowered regardless of the component. Conventionally, the remaining liquid in the distillation tank containing oil is removed when the number of times the workpiece has been cleaned reaches a predetermined number determined by empirical rules, but if the concentration of oil in the cleaning liquid after regeneration is measured, It is expected that the residual liquid can be removed at an appropriate timing.
 洗浄液の油分濃度を計測するために、例えば特許文献1に記載の方法を用いることが考えられる。特許文献1には、洗浄液に含有される油分の成分毎に定められた所定の一測定波長の紫外線を用いて吸光度を測定し、予め作成しておいた油分毎の油分濃度と吸光度の検量線に基づいて、その洗浄液に溶解している油分の濃度を求めることが記載されている。油分毎の測定波長は、例えば市販プレス油では259nm、市販切削油では234nm、市販フラックスでは250nmとされている。 In order to measure the oil concentration of the cleaning liquid, for example, the method described in Patent Document 1 can be used. In Patent Document 1, the absorbance is measured using ultraviolet light having a predetermined measurement wavelength determined for each component of the oil contained in the cleaning liquid, and a calibration curve of the oil concentration and the absorbance prepared in advance is prepared. Is used to determine the concentration of oil dissolved in the cleaning liquid. The measurement wavelength for each oil component is, for example, 259 nm for commercially available press oil, 234 nm for commercially available cutting oil, and 250 nm for commercially available flux.
特開平09-061349号公報JP 09-061349 A
 特許文献1に記載の油分濃度計測装置及び方法では、油分毎に測定波長が異なるため、それらの測定波長に対応して、複数の波長の光を検出しなければならない。そのためには例えば、それら複数の波長を含む光を試料(炭化水素系洗浄液)に照射する光源と、試料を通過した光を波長毎に分光する分光素子と、分光素子で分光された光を波長毎に検出する検出器を用いる。このような構成では、高価な光学素子である分光素子を用いる必要があるうえに、検出器にも波長毎に設けられた複数の検出素子を有する高価なものを用いる必要がある。また、波長毎にデータをほぼ同時に取得するため、短時間に大量のデータを処理及び保存するための高価な制御機器を要する。 In the oil concentration measuring device and method described in Patent Document 1, since the measurement wavelength differs for each oil component, light having a plurality of wavelengths must be detected corresponding to the measurement wavelengths. For that purpose, for example, a light source that irradiates the sample (hydrocarbon cleaning liquid) with light including a plurality of wavelengths, a spectroscopic element that splits the light that has passed through the sample for each wavelength, and a wavelength of the light that is split by the spectroscopic element A detector that detects each time is used. In such a configuration, it is necessary to use a spectroscopic element that is an expensive optical element, and it is also necessary to use an expensive detector having a plurality of detection elements provided for each wavelength. Moreover, since data is acquired almost simultaneously for each wavelength, an expensive control device for processing and storing a large amount of data in a short time is required.
 本発明が解決しようとする課題は、高価な分光素子、検出素子、及び制御機器を使用する必要がない、洗浄液中の油分濃度計測装置及び方法を提供することである。 The problem to be solved by the present invention is to provide an apparatus and a method for measuring the oil concentration in a cleaning liquid that do not require the use of expensive spectroscopic elements, detection elements, and control equipment.
 上記課題を解決するために成された本発明に係る洗浄液中の油分濃度計測装置は、
 a) 280~300nmの間の所定の1波長である測定波長を有する照射光を計測対象液に照射する光照射部と、
 b) 前記照射光が前記計測対象液を透過した透過光の強度を測定する透過光検出部と、
 c) 前記透過光検出部で測定された透過光の強度に基づき、前記計測対象液の前記測定波長における吸光度を算出し、該吸光度の値と、前記測定波長における油分の濃度と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める油分濃度決定部と
を備えることを特徴とする。
The oil concentration measuring device in the cleaning liquid according to the present invention made to solve the above problems,
a) a light irradiation unit for irradiating the measurement target liquid with irradiation light having a measurement wavelength which is a predetermined wavelength between 280 and 300 nm;
b) a transmitted light detector that measures the intensity of transmitted light through which the irradiation light has transmitted through the measurement target liquid;
c) Based on the intensity of the transmitted light measured by the transmitted light detection unit, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and the relationship between the absorbance value and the concentration of oil and absorbance at the measurement wavelength is calculated. And an oil concentration determination unit that obtains the concentration of the oil in the measurement target liquid based on a calibration curve that is shown.
 前述のように工業用洗浄機用の洗浄液として現在主流となっている炭化水素系洗浄液や、それ以外のグリコールエーテル系洗浄液等の多くの洗浄液は、炭素原子の多重(2重、3重)結合を有しない分子から成る。このような炭素原子の多重結合を有しない分子は、280nm未満の波長で吸光が生じる一方、280nm以上の波長ではほとんど吸光が生じない。それに対して、洗浄対象のワークに付着し、洗浄によって洗浄液に混入する切削油、プレス・打抜き油、機械油、グリース、フラックス等の油分のほとんどは炭素原子の多重結合を有する分子を含有する。このような炭素原子の多重結合を有する分子は、その種類によって吸光度がピークとなる波長は広い範囲に分布するが、油分の種類に依らず、280~300nmの波長範囲内において吸光度が0になることはなく一定の値を有する。さらに、波長が300nmを超えると、50ppm程度の低濃度の油分を検出することが困難になる。 As described above, many cleaning liquids such as hydrocarbon cleaning liquids, which are currently mainstream as cleaning liquids for industrial cleaning machines, and other glycol ether cleaning liquids, have multiple (double and triple) bonding of carbon atoms. It consists of molecules that do not have Molecules that do not have such multiple bonds of carbon atoms will absorb light at a wavelength of less than 280 nm, while light absorption will hardly occur at wavelengths of 280 nm or longer. On the other hand, most of oils such as cutting oil, press / punching oil, machine oil, grease, and flux that adhere to the workpiece to be cleaned and are mixed into the cleaning liquid by cleaning contain molecules having multiple bonds of carbon atoms. Molecules having such multiple bonds of carbon atoms have a broad range of wavelengths at which the absorbance peaks depending on the type, but the absorbance is 0 within the wavelength range of 280 to 300 nm regardless of the type of oil. It has a constant value. Furthermore, when the wavelength exceeds 300 nm, it becomes difficult to detect an oil component having a low concentration of about 50 ppm.
 そこで本発明では、280~300nmの間の所定の1波長である測定波長で透過光の強度を測定し、該強度に基づき該測定波長における吸光度を算出することにより、計測対象液(洗浄液、計測対象洗浄液)による吸光の影響を抑えつつ、該測定波長における測定対象の油分と吸光度の関係を示す検量線に基づいて当該油分の濃度を求めることができる。 Therefore, in the present invention, the intensity of transmitted light is measured at a measurement wavelength which is a predetermined one wavelength between 280 and 300 nm, and the absorbance at the measurement wavelength is calculated based on the intensity, whereby the measurement target liquid (cleaning liquid, measurement The concentration of the oil can be determined based on a calibration curve indicating the relationship between the oil content to be measured and the absorbance at the measurement wavelength while suppressing the influence of light absorption by the target cleaning solution.
 本発明に係る油分濃度計測装置によれば、測定波長として所定の1波長のみを用いるため、分光素子や波長毎の検出素子を用いる必要がない。また、複数の波長を用いる場合よりも同時に処理すべきデータ量が少ないため、高価な制御機器を使用する必要がない。例えば、本発明に係る油分濃度計測装置の専用の制御機器を設けることなく、工業用洗浄機が有する制御機器(プログラマブルロジックコントローラ)を用いて該油分濃度計測装置の制御を行うことができる。これらの理由により、本発明に係る油分濃度計測装置ではコストを抑えることができる。 According to the oil concentration measuring apparatus according to the present invention, since only one predetermined wavelength is used as the measurement wavelength, it is not necessary to use a spectroscopic element or a detection element for each wavelength. In addition, since the amount of data to be processed simultaneously is smaller than in the case of using a plurality of wavelengths, it is not necessary to use an expensive control device. For example, the oil concentration measuring device can be controlled using a control device (programmable logic controller) of an industrial washing machine without providing a dedicated control device for the oil concentration measuring device according to the present invention. For these reasons, the oil concentration measuring device according to the present invention can reduce the cost.
 本発明に係る油分濃度計測装置は、50~2000ppmという低濃度の油分の計測に好適に用いることができる。また、このような低濃度の油分の計測に適していることから、本発明に係る油分濃度計測装置は、50ppmという低濃度の油分を検出する能力が必要となる前述の蒸気洗浄・乾燥に用いられる再生後洗浄液中の油分濃度の計測に好適に用いることができる。なお、本発明に係る油分濃度計測装置による油分の計測の対象は、前記再生後洗浄液には限らず、例えばワークの洗浄中の洗浄槽において油分濃度の変化を計測することによって洗浄終了のタイミングを求める(油分濃度の時間変化が所定値以下になった時を終了のタイミングとする)ことに用いることもできる。 The oil concentration measuring apparatus according to the present invention can be suitably used for measuring oil components having a low concentration of 50 to 2000 ppm. In addition, since it is suitable for the measurement of such low-concentration oil content, the oil-concentration measurement device according to the present invention is used for the above-described steam cleaning / drying that requires the ability to detect a low-concentration oil content of 50 ppm. It can be suitably used for measuring the oil concentration in the post-regeneration cleaning liquid. Note that the target of oil content measurement by the oil concentration measuring device according to the present invention is not limited to the cleaning liquid after regeneration. It can also be used for obtaining (when the time change of the oil concentration becomes equal to or less than a predetermined value is set as the end timing).
 本発明に係る油分濃度計測装置はさらに、
 320~340nmの間の所定の1波長である第2測定波長を有する第2照射光を前記計測対象液に照射する第2光照射部と、
 前記第2照射光が前記計測対象液を透過した第2透過光の強度を測定する第2透過光検出部と、
 前記第2透過光検出部で測定された第2透過光の強度に基づき、前記計測対象液の前記第2測定波長における吸光度を算出し、該吸光度の値と、前記第2測定波長における油分の濃度と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める第2油分濃度決定部と
を備えていてもよい。
The oil concentration measuring device according to the present invention further includes:
A second light irradiation unit that irradiates the measurement target liquid with a second irradiation light having a second measurement wavelength that is a predetermined one wavelength between 320 and 340 nm;
A second transmitted light detector that measures the intensity of the second transmitted light through which the second irradiation light has passed through the measurement target liquid;
Based on the intensity of the second transmitted light measured by the second transmitted light detection unit, the absorbance at the second measurement wavelength of the measurement target liquid is calculated, and the value of the absorbance and the oil content at the second measurement wavelength are calculated. You may provide the 2nd oil concentration determination part which calculates | requires the density | concentration of the oil content in the said measurement object liquid based on the calibration curve which shows the relationship between a density | concentration and an absorbance.
 このように、280~300nmの間の所定の1波長である測定波長を有する照射光を用いた計測に加えて、320~340nmの間の所定の1波長である第2測定波長を有する第2照射光を用いて計測対象液(洗浄液、計測対象洗浄液)中の油分の濃度を求めることにより、吸光度がピークとなる波長が比較的長い油分における吸光度の測定精度を高くすることができる。この場合にも、油分の種類毎に異なる波長の光を用いる必要はなく、前記測定波長と前記第2測定波長の2種類の波長の光を用いるだけでよい。また、分光素子を用いる必要はなく、透過光の検出素子(透過光検出部及び第2透過光検出部)を多数設ける必要もない。さらには、前記照射光と前記第2照射光を互いに異なる時間に計測対象液に照射すれば、透過光を検出する検出器は、波長を認識する必要がないため、両波長に共通の1個の検出器を用いれば済む。このような検出器には、フォトダイオードを好適に用いることができる。 Thus, in addition to the measurement using the irradiation light having the measurement wavelength which is a predetermined one wavelength between 280 and 300 nm, the second having the second measurement wavelength which is a predetermined one wavelength between 320 and 340 nm. By determining the concentration of oil in the measurement target liquid (cleaning liquid, measurement target cleaning liquid) using the irradiation light, it is possible to increase the measurement accuracy of the absorbance of the oil having a relatively long wavelength at which the absorbance is peaked. Also in this case, it is not necessary to use different wavelengths of light for each type of oil, and it is only necessary to use light of two types of wavelengths, the measurement wavelength and the second measurement wavelength. Further, it is not necessary to use a spectroscopic element, and it is not necessary to provide a large number of transmitted light detection elements (transmitted light detection unit and second transmitted light detection unit). Furthermore, if the measurement target liquid is irradiated with the irradiation light and the second irradiation light at different times, the detector for detecting the transmitted light does not need to recognize the wavelength. This detector can be used. A photodiode can be suitably used for such a detector.
 本発明に係る洗浄液中の油分濃度計測方法は、
 280~300nmの間の所定の1波長である測定波長を有する照射光を計測対象液に照射し、
 前記照射光が前記計測対象液を透過した透過光の強度を測定し、
 前記透過光の強度に基づき、前記計測対象液の前記測定波長における吸光度を算出し、該吸光度の値と、前記測定波長における油分と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める
ことを特徴とする。
The method for measuring the oil concentration in the cleaning liquid according to the present invention is as follows.
Irradiate the measurement target liquid with irradiation light having a predetermined measurement wavelength of 280 to 300 nm,
Measure the intensity of transmitted light through which the irradiation light has passed through the measurement target liquid,
Based on the intensity of the transmitted light, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and based on the absorbance value and a calibration curve indicating the relationship between the oil content and the absorbance at the measurement wavelength, It is characterized by determining the concentration of oil.
 本発明により、高価な分光素子、検出素子、及び制御機器を使用する必要がなく安価な、洗浄液中の油分濃度計測装置及び方法を得ることができる。 According to the present invention, it is not necessary to use expensive spectroscopic elements, detection elements, and control equipment, and an inexpensive oil concentration measuring apparatus and method in a cleaning liquid can be obtained.
本発明に係る油分濃度計測装置の一実施形態を構成要素として有する工業用洗浄機を示す概略構成図。The schematic block diagram which shows the industrial washing machine which has one Embodiment of the oil concentration measuring apparatus which concerns on this invention as a component. 炭素原子の多重結合を有しない分子から成る4種の洗浄液における透過光量のスペクトルの測定値を示す図。The figure which shows the measured value of the spectrum of the transmitted light amount in four types of washing | cleaning liquid which consists of a molecule | numerator which does not have the multiple bond of a carbon atom. 本実施形態の油分濃度計測装置における制御部の機能を示す機能ブロック図。The functional block diagram which shows the function of the control part in the oil concentration measuring apparatus of this embodiment. 異なる4種類の油分をそれぞれ1種類ずつ含有する洗浄液の透過光量を測定した結果を示すグラフ。The graph which shows the result of having measured the transmitted light amount of the washing | cleaning liquid which contains one each of four different types of oil. 図4に示した透過光量から吸光度を求めた結果を示すグラフ。The graph which shows the result of having calculated | required the light absorbency from the transmitted light amount shown in FIG. 図5に示した吸光度に基づいて作成した油分毎の検量線を示すグラフ。6 is a graph showing a calibration curve for each oil component created based on the absorbance shown in FIG. 5. 本実施形態の油分濃度計測装置及び方法により洗浄液中の油分の濃度を測定した結果を示すグラフ。The graph which shows the result of having measured the density | concentration of the oil content in a washing | cleaning liquid with the oil content concentration measuring apparatus and method of this embodiment.
 図1~図7を用いて、本発明に係る油分濃度計測装置及び方法の実施形態を説明する。 Embodiments of an oil concentration measuring apparatus and method according to the present invention will be described with reference to FIGS.
 図1は、本実施形態の油分濃度計測装置10を構成要素として有する工業用洗浄機1の概略の構成を示している。工業用洗浄機1は、ワークに付着した油分を除去するための装置であり、油分濃度計測装置10の他に、第1洗浄槽11、第2洗浄槽12、蒸気洗浄・乾燥槽13、一時貯留槽14、蒸留槽15、熱交換器16、エゼクタ17、再生後洗浄液貯留槽18、試料セル洗浄液槽19を有する。図1中に示した太い実線は液体の流路を、太い破線は気体の流路を、細い直線の破線は電気信号の経路を、それぞれ示している。 FIG. 1 shows a schematic configuration of an industrial washing machine 1 having an oil concentration measuring device 10 of this embodiment as a component. The industrial cleaning machine 1 is a device for removing oil adhering to a workpiece. In addition to the oil concentration measuring device 10, the first cleaning tank 11, the second cleaning tank 12, the steam cleaning / drying tank 13, and the temporary It has a storage tank 14, a distillation tank 15, a heat exchanger 16, an ejector 17, a post-regeneration cleaning liquid storage tank 18, and a sample cell cleaning liquid tank 19. In FIG. 1, a thick solid line indicates a liquid flow path, a thick broken line indicates a gas flow path, and a thin straight broken line indicates an electric signal path.
(1) 工業用洗浄機1の全体構成及び動作
 本実施形態の油分濃度計測装置10について説明する前に、まず、工業用洗浄機1の全体構成及びワークの洗浄の動作を説明する。第1洗浄槽11及び第2洗浄槽12には、槽内に貯留される洗浄液に超音波振動を付与する超音波振動子が設けられている。また、超音波によるキャビテーションを生じ易くするために、第1洗浄槽11及び第2洗浄槽12内は真空ポンプにより減圧され、洗浄液の脱気が行われる。これら第1洗浄槽11及び第2洗浄槽12に洗浄液を貯留したうえで、ワークを洗浄液に浸漬し、超音波振動を付与することにより、ワークが洗浄される。ここで、後述の理由により、第1洗浄槽11内の洗浄液よりも第2洗浄槽12内の洗浄液の方が油分の含有量が少なくなることから、まず第1洗浄槽11でワークを洗浄し、次にそのワークを第2洗浄槽12で洗浄することにより、洗浄液中の油分がワークに再付着することを最小限に抑えることができる。
(1) Overall Configuration and Operation of Industrial Cleaning Machine 1 Before describing the oil concentration measuring apparatus 10 of the present embodiment, first, the overall configuration of the industrial cleaning machine 1 and the operation of cleaning the workpiece will be described. The first cleaning tank 11 and the second cleaning tank 12 are provided with an ultrasonic vibrator that applies ultrasonic vibration to the cleaning liquid stored in the tank. Moreover, in order to make it easy to produce cavitation by an ultrasonic wave, the inside of the 1st washing tank 11 and the 2nd washing tank 12 is pressure-reduced with a vacuum pump, and deaeration of a washing | cleaning liquid is performed. After storing the cleaning liquid in the first cleaning tank 11 and the second cleaning tank 12, the work is cleaned by immersing the work in the cleaning liquid and applying ultrasonic vibration. Here, for the reason described later, since the oil content of the cleaning liquid in the second cleaning tank 12 is smaller than the cleaning liquid in the first cleaning tank 11, the work is first cleaned in the first cleaning tank 11. Then, by cleaning the workpiece in the second cleaning tank 12, it is possible to minimize the oil in the cleaning liquid from reattaching to the workpiece.
 蒸気洗浄・乾燥槽13は、第2洗浄槽12で洗浄されたワークに対して蒸気洗浄及び乾燥を行うための槽である。蒸気洗浄・乾燥に使用される蒸気は、後述のように蒸留槽15から供給される。蒸気洗浄・乾燥槽13内の蒸気、及びワークの表面に残留していたものが除去された洗浄液は、第2洗浄槽12に返送される。また、第1洗浄槽11及び第2洗浄槽12の減圧や洗浄液の蒸発により生じた気体は、一時貯留槽14に回収される。 The steam cleaning / drying tank 13 is a tank for performing steam cleaning and drying on the workpiece cleaned in the second cleaning tank 12. The steam used for steam cleaning / drying is supplied from the distillation tank 15 as described later. The cleaning liquid from which the steam in the steam cleaning / drying tank 13 and the material remaining on the surface of the work are removed is returned to the second cleaning tank 12. Further, the gas generated by the decompression of the first cleaning tank 11 and the second cleaning tank 12 and the evaporation of the cleaning liquid is collected in the temporary storage tank 14.
 蒸留槽15にはフロート弁151が設けられており、蒸留槽15内の液体が蒸留により所定量以下になると、洗浄液が一時貯留槽14から蒸留槽15内に導入される。蒸留槽15内にはヒータ(図示せず)により加熱されると共に、エゼクタ17により減圧される。これにより、洗浄液は油分を液体として残して蒸発する。発生した蒸気の一部は前述のように蒸気洗浄・乾燥槽13に供給され、残りは熱交換器16で凝縮されたうえで、再生後洗浄液貯留槽18に貯留される。 The distillation tank 15 is provided with a float valve 151, and when the liquid in the distillation tank 15 becomes a predetermined amount or less by distillation, the cleaning liquid is introduced from the temporary storage tank 14 into the distillation tank 15. The distillation tank 15 is heated by a heater (not shown) and depressurized by an ejector 17. As a result, the cleaning liquid evaporates leaving the oil as a liquid. A part of the generated steam is supplied to the steam cleaning / drying tank 13 as described above, and the rest is condensed in the heat exchanger 16 and then stored in the cleaning liquid storage tank 18 after regeneration.
 第2洗浄槽12には、蒸留槽15によって油分が除去された再生後洗浄液が再生後洗浄液貯留槽18から流入する。第1洗浄槽11と第2洗浄槽12は第2オーバーフロー管122で接続されている。第2オーバーフロー管122は、第1洗浄槽11との接続位置よりも第2洗浄槽12との接続位置の方が高くなっており、再生後洗浄液の流入によって第2洗浄槽12内の洗浄液の液面が後者の接続位置よりも高くなると、第2洗浄槽12内の洗浄液の一部が自然に第1洗浄槽11に移動する。従って、第1洗浄槽11内の洗浄液よりも第2洗浄槽12内の洗浄液の方が油分の含有量が少なくなる。また、第1洗浄槽11と一時貯留槽14は第1オーバーフロー管112で接続されており、第2洗浄槽12からの洗浄液の流入によって第1洗浄槽11内の洗浄液の液面が第1オーバーフロー管112の接続位置よりも高くなると、第1洗浄槽11中の洗浄液の一部が自然に第1オーバーフロー管112を通って一時貯留槽14に移動する。 The post-regeneration cleaning liquid from which oil has been removed by the distillation tank 15 flows from the post-regeneration cleaning liquid storage tank 18 into the second cleaning tank 12. The first cleaning tank 11 and the second cleaning tank 12 are connected by a second overflow pipe 122. The second overflow pipe 122 has a higher connection position with the second cleaning tank 12 than a connection position with the first cleaning tank 11, and the cleaning liquid in the second cleaning tank 12 flows due to the inflow of the cleaning liquid after regeneration. When the liquid level becomes higher than the latter connection position, a part of the cleaning liquid in the second cleaning tank 12 naturally moves to the first cleaning tank 11. Accordingly, the cleaning liquid in the second cleaning tank 12 has a smaller oil content than the cleaning liquid in the first cleaning tank 11. Further, the first cleaning tank 11 and the temporary storage tank 14 are connected by a first overflow pipe 112, and the liquid level of the cleaning liquid in the first cleaning tank 11 is caused by the inflow of the cleaning liquid from the second cleaning tank 12. If it becomes higher than the connection position of the pipe | tube 112, a part of washing | cleaning liquid in the 1st washing tank 11 will move to the temporary storage tank 14 through the 1st overflow pipe 112 naturally.
 第1洗浄槽11は、洗浄液を槽内から取り出し、フィルタを通して槽内に戻す第1循環濾過系111を有する。第2洗浄槽12にも同様の第2循環濾過系121が設けられている。これら循環濾過系は、粒径10μm程度以上のパーティクルを除去するものであって、油分を除去することができない。 The 1st washing tank 11 has the 1st circulation filtration system 111 which takes out cleaning fluid from a tank, and returns it in a tank through a filter. A similar second circulation filtration system 121 is also provided in the second cleaning tank 12. These circulating filtration systems remove particles having a particle size of about 10 μm or more, and cannot remove oil.
(2) 本実施形態の油分濃度計測装置10の構成
 次に、工業用洗浄機1中の油分濃度計測装置10の構成について詳細に説明する。油分濃度計測装置10は、後述のように第1洗浄槽11、第2洗浄槽12及び再生後洗浄液貯留槽18と接続される流路101と、流路101中に設けられた送液ポンプ102と、流路101中の送液ポンプ102よりも下流側に設けられた試料セル103と、リファレンス測定用のリファレンスセル1031と、光照射部104と、透過光検出部105と、装置全体の制御や後述のデータ処理を行う制御部106を有する。
(2) Configuration of Oil Concentration Measuring Device 10 of this Embodiment Next, the configuration of the oil concentration measuring device 10 in the industrial cleaning machine 1 will be described in detail. The oil concentration measuring apparatus 10 includes a flow path 101 connected to the first cleaning tank 11, the second cleaning tank 12, and the post-regeneration cleaning liquid storage tank 18, and a liquid feed pump 102 provided in the flow path 101, as will be described later. And a sample cell 103 provided downstream of the liquid feed pump 102 in the flow channel 101, a reference cell 1031 for reference measurement, a light irradiation unit 104, a transmitted light detection unit 105, and control of the entire apparatus. And a control unit 106 that performs data processing to be described later.
 流路101の流入部1011は、第1中継管113を介して第1洗浄槽11に、第2中継管123を介して第2洗浄槽12に、第3中継管183を介して再生後洗浄液貯留槽18に、それぞれ接続されている。また、第1中継管113には第1中継開閉弁11Vが、第2中継管123には第2中継開閉弁12Vが、第3中継管183には第3中継開閉弁18Vが、それぞれ設けられている。 The inflow portion 1011 of the flow path 101 is supplied to the first cleaning tank 11 via the first relay pipe 113, to the second cleaning tank 12 via the second relay pipe 123, and after-regeneration cleaning liquid via the third relay pipe 183. Each is connected to the storage tank 18. The first relay pipe 113 is provided with a first relay on-off valve 11V, the second relay pipe 123 is provided with a second relay on-off valve 12V, and the third relay pipe 183 is provided with a third relay on-off valve 18V. ing.
 流路101の流出部は一時貯留槽14に接続されている。従って、油分濃度計測装置10において測定に用いられた洗浄液は、一時貯留槽14を経て蒸留槽15により蒸留され、最終的には油分が除去された状態で第2洗浄槽12に返送される。なお、測定に用いられた洗浄液を流出部から、その洗浄液が収容されていた槽に直接返送するようにしてもよい。 The outflow part of the channel 101 is connected to the temporary storage tank 14. Therefore, the cleaning liquid used for the measurement in the oil concentration measuring device 10 is distilled by the distillation tank 15 through the temporary storage tank 14, and finally returned to the second cleaning tank 12 in a state where the oil is removed. In addition, you may make it return the washing | cleaning liquid used for the measurement directly from the outflow part to the tank in which the washing | cleaning liquid was accommodated.
 試料セル103及びリファレンスセル1031はいずれも、紫外線の吸収が少ない石英製のセルである。流路101には、通常の測定時には試料セル103が接続され、リファレンスデータを測定する時にはリファレンスセル1031が接続される。リファレンスセル1031には、油分を含まない洗浄液が封入されており、制御部106による制御により、所定の時間間隔で油分濃度の測定を中断したうえでリファレンスデータを測定するようになっている。 Both the sample cell 103 and the reference cell 1031 are quartz cells that absorb less ultraviolet light. The sample cell 103 is connected to the channel 101 during normal measurement, and the reference cell 1031 is connected when measuring reference data. The reference cell 1031 is filled with a cleaning liquid that does not contain oil, and the reference data is measured after interrupting the measurement of the oil concentration at predetermined time intervals under the control of the control unit 106.
 光照射部104は、本実施形態では280~300nmの間の所定の1波長である測定波長を試料セル103内の洗浄液(計測対象液)に照射するものであり、当該測定波長を発光するLEDから成る。本実施形態では、測定波長は290nmとした。 In the present embodiment, the light irradiation unit 104 irradiates the cleaning liquid (measurement target liquid) in the sample cell 103 with a predetermined measurement wavelength between 280 and 300 nm, and emits the measurement wavelength. Consists of. In this embodiment, the measurement wavelength is 290 nm.
 ここで図2を用いて、測定波長を280~300nmの間の1波長とする理由を説明する。図2は、炭素原子の多重結合を有しない分子から成る4種の洗浄液1~4における透過光量のスペクトルの測定値を示している。4種のうち洗浄液1~3はいずれも飽和型脂肪族炭化水素系の洗浄液であり、洗浄液4はグリコールエーテル系の洗浄液である。図2には合わせて、入射光のスペクトルを示す。4種の洗浄液はいずれも波長280nm未満において透過光量が入射光の光量よりも大幅に小さくなっており、洗浄液による紫外線の吸収が見られる。それに対して波長280nm以上では、透過光量と入射光の差が小さく、洗浄液による紫外線の吸収がほとんど無い。従って、280nmの測定波長で測定すれば、洗浄液による吸光の影響を抑えつつ油分の濃度の計測を行うことができる。一方、測定波長が300nmを超えると、後掲の図5に示すように、低濃度(図5に示した例では100ppm。さらには50ppm。)の油分による吸光度の値が小さくなりすぎるため求めることができない。従って、280~300nmの間の1波長を測定波長とすることにより、洗浄液による吸光の影響を抑えつつ、50ppm程度の低濃度であっても油分の濃度の計測を行うことができる。 Here, the reason why the measurement wavelength is set to one wavelength between 280 and 300 nm will be described with reference to FIG. FIG. 2 shows measured values of the spectrum of transmitted light in the four types of cleaning liquids 1 to 4 composed of molecules having no multiple bonds of carbon atoms. Of the four types, cleaning solutions 1 to 3 are all saturated aliphatic hydrocarbon cleaning solutions, and cleaning solution 4 is a glycol ether cleaning solution. FIG. 2 also shows the spectrum of incident light. All of the four types of cleaning liquids have a transmitted light amount that is significantly smaller than the amount of incident light at a wavelength of less than 280 nm, and ultraviolet light is absorbed by the cleaning liquid. On the other hand, when the wavelength is 280 nm or more, the difference between the transmitted light amount and the incident light is small, and the ultraviolet rays are hardly absorbed by the cleaning liquid. Therefore, if the measurement is performed at a measurement wavelength of 280 nm, the concentration of the oil can be measured while suppressing the influence of light absorption by the cleaning liquid. On the other hand, when the measurement wavelength exceeds 300 nm, as shown in FIG. 5 to be described later, the absorbance value due to the oil component at a low concentration (100 ppm in the example shown in FIG. 5 and further 50 ppm) becomes too small. I can't. Therefore, by setting one wavelength between 280 and 300 nm as the measurement wavelength, it is possible to measure the oil concentration even at a low concentration of about 50 ppm while suppressing the influence of light absorption by the cleaning liquid.
 透過光検出部105は、試料セル103内の洗浄液を透過した前記測定波長を有する透過光の強度を検出するものであり、フォトダイオードと信号変換部から成る。フォトダイオードは前記測定波長の光を検出してその強度をアナログ信号として出力する。信号変換部は、フォトダイオードが出力したアナログ信号をデジタル信号に変換する。 The transmitted light detection unit 105 detects the intensity of transmitted light having the measurement wavelength that has passed through the cleaning liquid in the sample cell 103, and includes a photodiode and a signal conversion unit. The photodiode detects the light of the measurement wavelength and outputs the intensity as an analog signal. The signal converter converts the analog signal output from the photodiode into a digital signal.
 制御部106は、図3の機能ブロック図に示す機能を有する。制御部106には、プログラマブルロジックコントローラやパーソナルコンピュータを用いることができ、工業用洗浄機が有する制御装置をそのまま適用してもよいし、油分濃度計測装置10の制御装置を備えるようにしてもよい。制御部106は、油分濃度決定部1061と、リファレンスデータ記録部1062と、検量線記録部1063と、条件入力部1064と、測定制御部1065を有する。油分濃度決定部1061は、吸光度算出部1061Aと、検量線選択部1061Bと、検量線適用部1061Cから構成される。油分濃度決定部1061の詳細は、本実施形態の油分濃度計測装置10の動作と共に後述する。リファレンスデータ記録部1062には、油分を含有しない洗浄剤について予め測定された、前記測定波長における透過光量のデータ(リファレンスデータ)が記録されている。検量線記録部1063には、ワークの加工に使用し得る油分毎に、油分の濃度が既知である試料を用いて予め測定したデータに基づいて作成された、前記測定波長における油分の濃度と吸光度の関係を示す検量線が記録されている。なお、メーカや型番が異なる複数の加工油同士で成分が近い場合には、それら複数の加工油で共通の検量線を用いてもよい。条件入力部1064は、測定者がタッチパネル等の入力デバイスを用いて後述の測定条件を入力するものである。測定制御部1065は、光照射部104における光源からの光の照射の開始及び終了や、上記各部の処理の開始及び終了等の制御を行う。 The control unit 106 has the functions shown in the functional block diagram of FIG. As the control unit 106, a programmable logic controller or a personal computer can be used, and a control device of an industrial cleaning machine may be applied as it is, or a control device of the oil concentration measuring device 10 may be provided. . The control unit 106 includes an oil concentration determination unit 1061, a reference data recording unit 1062, a calibration curve recording unit 1063, a condition input unit 1064, and a measurement control unit 1065. The oil concentration determination unit 1061 includes an absorbance calculation unit 1061A, a calibration curve selection unit 1061B, and a calibration curve application unit 1061C. Details of the oil concentration determination unit 1061 will be described later together with the operation of the oil concentration measuring apparatus 10 of the present embodiment. The reference data recording unit 1062 records transmitted light amount data (reference data) at the measurement wavelength, which is measured in advance for a cleaning agent that does not contain oil. The calibration curve recording unit 1063 includes, for each oil component that can be used for processing the workpiece, the concentration and absorbance of the oil component at the measurement wavelength created based on data measured in advance using a sample having a known oil component concentration. A calibration curve showing the relationship is recorded. In addition, when components are close to each other between a plurality of processing oils having different manufacturers and model numbers, a common calibration curve may be used for the plurality of processing oils. The condition input unit 1064 is used by the measurer to input measurement conditions described later using an input device such as a touch panel. The measurement control unit 1065 controls the start and end of light irradiation from the light source in the light irradiation unit 104 and the start and end of the processing of each unit.
 試料セル洗浄液槽19は、試料セル103を洗浄するための洗浄液(油分濃度計測の対象である洗浄液と同じもの)が貯留される槽である。 The sample cell cleaning liquid tank 19 is a tank in which a cleaning liquid for cleaning the sample cell 103 (the same as the cleaning liquid that is the target of oil concentration measurement) is stored.
(3) 本実施形態の油分濃度計測装置10の動作
 本実施例の油分濃度計測装置10の動作を説明する。ここでは主に、蒸気洗浄・乾燥槽13で使用される蒸気中の油分濃度に近い、再生後洗浄液貯留槽18内に貯留されている再生後洗浄液を油分濃度の測定対象とする場合について述べる。
(3) Operation of Oil Concentration Measuring Device 10 of the Present Embodiment The operation of the oil concentration measuring device 10 of the present embodiment will be described. Here, a case will be mainly described in which the post-regeneration cleaning liquid stored in the post-regeneration cleaning liquid storage tank 18 that is close to the oil concentration in the steam used in the steam cleaning / drying tank 13 is an oil concentration measurement target.
 まず、測定者が条件入力部1064において所定の測定条件を入力したうえで、測定開始の指示を入力することにより、測定が開始される。ここで入力される測定条件は、測定対象の洗浄液を用いて洗浄されるワークに付着していた加工油を特定するための情報(例えば加工油のメーカ及び型番)である。 First, measurement is started when the measurer inputs a predetermined measurement condition in the condition input unit 1064 and then inputs a measurement start instruction. The measurement condition input here is information (for example, manufacturer and model number of the processing oil) for specifying the processing oil attached to the workpiece to be cleaned using the cleaning liquid to be measured.
 測定が開始されると、まず、測定対象の洗浄液が貯留されている洗浄槽あるいは貯留槽に対応する中継弁が開放される。ここでは、再生後洗浄液貯留槽18に接続されている第3中継管183に設けられた第3中継開閉弁18Vを開放する。これにより、測定対象の再生後洗浄液が流路101を通って試料セル103に導入される。なお、測定対象の洗浄液が第1洗浄槽11内の洗浄液であれば第1中継開閉弁11Vを開放し、第2洗浄槽12内の洗浄液であれば第2中継開閉弁12Vを開放する。 When measurement is started, first, the cleaning tank storing the cleaning liquid to be measured or the relay valve corresponding to the storage tank is opened. Here, the third relay open / close valve 18V provided in the third relay pipe 183 connected to the post-regeneration cleaning liquid storage tank 18 is opened. As a result, the post-regeneration cleaning liquid to be measured is introduced into the sample cell 103 through the channel 101. If the cleaning liquid to be measured is the cleaning liquid in the first cleaning tank 11, the first relay on / off valve 11V is opened, and if the cleaning liquid in the second cleaning tank 12 is to be opened, the second relay on / off valve 12V is opened.
 光照射部104は試料セル103内の洗浄液に対して前記測定波長(290nm)の光を照射する。透過光検出部105は、洗浄液を透過した透過光量の強度Iを測定し、デジタル信号に変換して出力する。 The light irradiation unit 104 irradiates the cleaning liquid in the sample cell 103 with light having the measurement wavelength (290 nm). The transmitted light detection unit 105 measures the intensity I of the transmitted light amount that has passed through the cleaning liquid, converts it into a digital signal, and outputs it.
 次に、制御部106は、透過光検出部105から出力された透過光量の強度Iを示すデジタル信号を入力すると共に、リファレンスデータ記録部1062から、油分を含有しない洗浄液の前記測定波長における透過光量であるリファレンスデータI0を取得する。制御部106の吸光度算出部1061Aは、これら測定対象の洗浄液における透過光量の強度IとリファレンスデータI0に基づいて、測定対象の洗浄液の吸光度A=log10(I0/I)を求める。 Next, the control unit 106 inputs a digital signal indicating the intensity I of the transmitted light amount output from the transmitted light detection unit 105 and transmits the transmitted light amount at the measurement wavelength of the cleaning liquid not containing oil from the reference data recording unit 1062. Reference data I 0 is acquired. The absorbance calculation unit 1061A of the control unit 106 obtains the absorbance A = log 10 (I 0 / I) of the cleaning liquid to be measured based on the transmitted light intensity I in the cleaning liquid to be measured and the reference data I 0 .
 続いて、制御部106の検量線選択部1061Bは、条件入力部1064で入力された加工油を特定するための情報に基づいて、特定された加工油に対応する検量線を検量線記録部1063から取得する。そして、検量線適用部1061Cは、吸光度算出部1061Aで得られた測定対象の洗浄液の吸光度Aを、検量線選択部1061Bで選択された検量線に適用し、加工油の濃度を求める。 Subsequently, the calibration curve selection unit 1061B of the control unit 106 generates a calibration curve corresponding to the specified processing oil based on the information for specifying the processing oil input by the condition input unit 1064. Get from. Then, the calibration curve application unit 1061C applies the absorbance A of the cleaning liquid to be measured obtained by the absorbance calculation unit 1061A to the calibration curve selected by the calibration curve selection unit 1061B, and obtains the concentration of the processing oil.
 以後、測定対象の再生後洗浄液を連続的に試料セル103に導入しつつ、光照射部104による光の照射及び透過光量の強度Iの測定を繰り返し行うことにより、加工油の濃度を繰り返し求める。そして、加工油の濃度が所定値を超えたときには、蒸留槽15内に残留する残留液の処理を行う。残留液の処理は、残留液を煮詰めることにより残留液中の洗浄液と加工油を分離し、これにより蒸留槽15内に残留した加工油を廃棄することにより行う。 Thereafter, the concentration of the processing oil is repeatedly obtained by repeatedly introducing the cleaning liquid after regeneration to the sample cell 103 into the sample cell 103 and repeatedly performing the light irradiation by the light irradiation unit 104 and the measurement of the intensity I of the transmitted light amount. When the concentration of the processing oil exceeds a predetermined value, the residual liquid remaining in the distillation tank 15 is processed. The treatment of the residual liquid is performed by separating the cleaning liquid and the processing oil in the residual liquid by boiling the residual liquid, thereby discarding the processing oil remaining in the distillation tank 15.
 なお、測定対象の洗浄液が第1洗浄槽11内又は第2洗浄槽12内の洗浄液とする場合には、ワークの洗浄中に上記と同様の方法により洗浄液中の加工油の濃度を繰り返し求め、その濃度の時間変化が所定値以下になった時にワークの洗浄を終了するという、洗浄終了のタイミングを求めるために測定結果を用いることができる。 When the cleaning liquid to be measured is the cleaning liquid in the first cleaning tank 11 or the second cleaning tank 12, the concentration of the processing oil in the cleaning liquid is repeatedly obtained by the same method as described above during the cleaning of the workpiece. The measurement result can be used to determine the timing of completion of cleaning, that is, the cleaning of the workpiece is terminated when the change with time of the concentration becomes a predetermined value or less.
(4) 吸光度及び検量線の例
 代表的な加工油として選択した4種類の油分(表1)をそれぞれ、同じ洗浄液に異なる濃度で混合した複数の試料を作製し、油分及び濃度毎の透過光量を測定して吸光度を求めた。ここでは、測定波長を290nmとすることの妥当性を検証するために、波長を290nmには限定せずに260~400nmの範囲内で透過光量の測定を行った。ここで洗浄液には、炭素原子の多重結合を有しない飽和型脂肪族炭化水素系の洗浄液である「NS100」(JXエネルギー(株)製、図2の洗浄液1)を用いた。また、各油分の濃度はいずれも、100ppm、500ppm、2000ppm及び10000ppmとした。
Figure JPOXMLDOC01-appb-T000001
(4) Absorbance and calibration curve examples Prepare multiple samples of four types of oil (Table 1) selected as typical processing oils in the same cleaning solution at different concentrations, and transmit light quantity for each oil and concentration. Was measured to determine the absorbance. Here, in order to verify the validity of setting the measurement wavelength to 290 nm, the amount of transmitted light was measured within the range of 260 to 400 nm without limiting the wavelength to 290 nm. Here, “NS100” (manufactured by JX Energy Co., Ltd., cleaning liquid 1 in FIG. 2), which is a saturated aliphatic hydrocarbon-based cleaning liquid having no multiple bonds of carbon atoms, was used as the cleaning liquid. In addition, the concentration of each oil was 100 ppm, 500 ppm, 2000 ppm, and 10000 ppm.
Figure JPOXMLDOC01-appb-T000001
 測定により得られた透過光量を、洗浄液が含有する油分毎に図4に示す。また、図4に示した透過光量に基づいて吸光度を求めた結果を図5に示す。いずれも、波長280~300nmの範囲内において、吸光度が油分の濃度に依存して異なる値を有している。 The amount of transmitted light obtained by the measurement is shown in FIG. 4 for each oil contained in the cleaning liquid. Moreover, the result of having calculated | required the light absorbency based on the transmitted light amount shown in FIG. 4 is shown in FIG. In any case, within the wavelength range of 280 to 300 nm, the absorbance has a different value depending on the oil concentration.
 こうして得られた、波長290nmにおける油分及び濃度毎の吸光度に基づき、油分毎に、吸光度と濃度の関係を示す検量線を作成した。作成した検量線を図6に示す。なお、各油分において、濃度が10000ppmのデータは検量線において直線から外れるため使用していない。図6に示すように、濃度が2000ppm以下のときには検量線を直線で示すことができる。従って、少なくとも2000ppm以下の濃度において、本実施形態の油分濃度計測装置及び方法による油分濃度の計測が可能である。 Based on the oil content at a wavelength of 290 nm and the absorbance at each concentration thus obtained, a calibration curve showing the relationship between the absorbance and the concentration was prepared for each oil content. The prepared calibration curve is shown in FIG. For each oil, data with a concentration of 10,000 ppm is not used because it deviates from the straight line in the calibration curve. As shown in FIG. 6, when the concentration is 2000 ppm or less, the calibration curve can be shown as a straight line. Therefore, at a concentration of at least 2000 ppm, the oil concentration can be measured by the oil concentration measuring apparatus and method of this embodiment.
 図1に示した工業用洗浄機において、ワークの洗浄の品質を維持するために重要なことは、蒸留槽15で蒸留再生される再生後洗浄液の油分の濃度を計測・管理することである。特に、再生後洗浄液は、蒸留槽15で発生した蒸気がそのまま蒸気洗浄・乾燥槽13においてワークに対する仕上げの洗浄である蒸気洗浄に用いられるため、油分濃度の計測・管理を工業用洗浄機の連続運転中に行うことが最も重要である。本発明によれば、このような工業用洗浄機の連続運転中ににおける油分濃度の計測・管理が可能である。 In the industrial washer shown in FIG. 1, it is important to measure and manage the oil concentration of the regenerated cleaning liquid that is distilled and regenerated in the distillation tank 15 in order to maintain the quality of workpiece cleaning. In particular, since the steam generated in the distillation tank 15 is used as it is in the steam cleaning / drying tank 13 for steam cleaning, which is the finishing cleaning of the workpiece, the oil concentration is measured and managed continuously by an industrial cleaning machine. Most important to do while driving. According to the present invention, it is possible to measure and manage the oil concentration during continuous operation of such an industrial washer.
 得られた検量線を用いて、再生後洗浄液中の油分の濃度を計測する実験を行った。この実験においても、洗浄液は上記NS100、又はNS200(JXエネルギー(株)製、図2の洗浄液2)を用い、添加する油分には上掲の表1に示したものを含む、5種類の切削油及び5種類のプレス・打ち抜き油を用いた。この実験では、洗浄液及び油分を秤量したうえで両者を混合することにより、濃度が既知(この濃度を「本来の濃度」と呼ぶ)である試料を作製し、本来の濃度と測定値の比較を行った。 Using the obtained calibration curve, an experiment was conducted to measure the concentration of oil in the cleaning liquid after regeneration. Also in this experiment, the above-mentioned NS100 or NS200 (manufactured by JX Energy Co., Ltd., cleaning liquid 2 in FIG. 2) was used as the cleaning liquid, and the oils to be added included five types of cutting including those shown in Table 1 above. Oil and 5 kinds of press and punching oil were used. In this experiment, a sample with a known concentration (this concentration is referred to as the “original concentration”) is prepared by weighing the cleaning solution and the oil and mixing them, and then comparing the original concentration with the measured value. went.
 実験結果を図7のグラフに示す。このグラフでは、本来の濃度を横軸に、測定値を縦軸にとった。データ点は、測定値が本来の濃度の±10%以内に収まれば、グラフ中の2本の破線の間に収まる。また、図7では、全ての試料をデータを1つのグラフに掲載した。このグラフに示すように、今回得られた全ての測定値が概ね本来の濃度の±10%以内に収まっている。±10%程度の精度があれば、工業用洗浄機において用いるには十分である。 The experimental results are shown in the graph of FIG. In this graph, the original concentration is plotted on the horizontal axis and the measured value is plotted on the vertical axis. The data point falls between the two dashed lines in the graph if the measured value is within ± 10% of the original concentration. In FIG. 7, data for all samples are shown in one graph. As shown in this graph, all the measured values obtained this time are generally within ± 10% of the original concentration. An accuracy of about ± 10% is sufficient for use in industrial washing machines.
(5) 変形例
 本実施形態の油分濃度計測装置10において、光照射部104は、波長280~300nmの間の測定波長(上記の例では290nm)の光を洗浄液に照射する他に、320~340nmの間の所定の1波長である第2測定波長を洗浄液に照射するようにしてもよい。このような異なる2つの波長の光は、単色光を発する光源であって該単色光の波長が異なる2つの光源を用いて生成することが望ましい。この場合、透過光検出部105は、上記測定波長の光と第2測定波長の光の双方の強度を測定できるものであれば、これら2つの波長の光を共通に検出するものとして1つのみあればよい。あるいは、波長毎に異なる透過光検出部を用いてもよい。当該第2測定波長においても前記測定波長(290nm)の場合と同様に、図5の吸光度のデータに基づいて、油分毎に、吸光度と濃度の関係を示す検量線を作成することができる。
(5) Modification In the oil concentration measuring apparatus 10 of the present embodiment, the light irradiation unit 104 irradiates the cleaning liquid with light having a measurement wavelength between 280 and 300 nm (290 nm in the above example). The cleaning liquid may be irradiated with a second measurement wavelength that is a predetermined wavelength of 340 nm. Such two different wavelengths of light are preferably generated using two light sources that emit monochromatic light and have different wavelengths of monochromatic light. In this case, as long as the transmitted light detection unit 105 can measure the intensities of both the light having the measurement wavelength and the light having the second measurement wavelength, only one light can be detected in common. I just need it. Or you may use the transmitted light detection part which changes for every wavelength. Similarly to the case of the measurement wavelength (290 nm), a calibration curve showing the relationship between absorbance and concentration can be created for each oil component based on the absorbance data in FIG.
 例えば、図6(d)に示した検量線は、(a)~(c)の検量線と比較して、吸光度を求めた点と検量線との差がやや大きいことから、2つの測定波長でそれぞれ油分の濃度を求めることにより、精度を高くすることができる。 For example, the calibration curve shown in Fig. 6 (d) has a slightly larger difference between the point where the absorbance was obtained and the calibration curve than the calibration curves (a) to (c). Thus, the accuracy can be increased by obtaining the oil concentration.
1…工業用洗浄機
10…油分濃度計測装置
101…流路
1011…流入部
102…送液ポンプ
103…試料セル
1031…リファレンスセル
104…光照射部
105…透過光検出部
106…制御部
1061…油分濃度決定部
1061A…吸光度算出部
1061B…検量線選択部
1061C…検量線適用部
1062…リファレンスデータ記録部
1063…検量線記録部
1064…条件入力部
1065…測定制御部
11…第1洗浄槽
111…第1循環濾過系
112…第1オーバーフロー管
113…第1中継管
11V…第1中継開閉弁
12…第2洗浄槽
121…第2循環濾過系
122…第2オーバーフロー管
123…第2中継管
12V…第2中継開閉弁
13…蒸気洗浄・乾燥槽
14…一時貯留槽
15…蒸留槽
151…フロート弁
16…熱交換器
17…エゼクタ
18…再生後洗浄液貯留槽
183…第3中継管
18V…第3中継開閉弁
19…試料セル洗浄液槽
DESCRIPTION OF SYMBOLS 1 ... Industrial washing machine 10 ... Oil concentration measuring device 101 ... Flow path 1011 ... Inflow part 102 ... Liquid feeding pump 103 ... Sample cell 1031 ... Reference cell 104 ... Light irradiation part 105 ... Transmitted light detection part 106 ... Control part 1061 ... Oil concentration determination unit 1061A ... absorbance calculation unit 1061B ... calibration curve selection unit 1061C ... calibration curve application unit 1062 ... reference data recording unit 1063 ... calibration curve recording unit 1064 ... condition input unit 1065 ... measurement control unit 11 ... first cleaning tank 111 ... 1st circulation filtration system 112 ... 1st overflow pipe 113 ... 1st relay pipe 11V ... 1st relay on-off valve 12 ... 2nd washing tank 121 ... 2nd circulation filtration system 122 ... 2nd overflow pipe 123 ... 2nd relay pipe 12V ... second relay opening / closing valve 13 ... steam cleaning / drying tank 14 ... temporary storage tank 15 ... distillation tank 151 ... float valve 16 ... heat exchanger 17 Ejector 18 ... playback after the cleaning liquid storage tank 183 ... third relay pipe 18V ... third relay off valve 19 ... sample cell washing solution tank

Claims (5)

  1.  a) 280~300nmの間の所定の1波長である測定波長を有する照射光を計測対象液に照射する光照射部と、
     b) 前記照射光が前記計測対象液を透過した透過光の強度を測定する透過光検出部と、
     c) 前記透過光検出部で測定された透過光の強度に基づき、前記計測対象液の前記測定波長における吸光度を算出し、該吸光度の値と、前記測定波長における油分の濃度と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める油分濃度決定部と
    を備えることを特徴とする、洗浄液中の油分濃度計測装置。
    a) a light irradiation unit for irradiating the measurement target liquid with irradiation light having a measurement wavelength which is a predetermined wavelength between 280 and 300 nm;
    b) a transmitted light detector that measures the intensity of transmitted light through which the irradiation light has transmitted through the measurement target liquid;
    c) Based on the intensity of the transmitted light measured by the transmitted light detection unit, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and the relationship between the absorbance value and the concentration of oil and absorbance at the measurement wavelength is calculated. An oil concentration measuring device in cleaning liquid, comprising: an oil concentration determining unit that obtains the concentration of oil in the measurement target liquid based on a calibration curve that is shown.
  2.  さらに、
     320~340nmの間の所定の1波長である第2測定波長を有する第2照射光を前記計測対象液に照射する第2光照射部と、
     前記第2照射光が前記計測対象液を透過した第2透過光の強度を測定する第2透過光検出部と、
     前記第2透過光検出部で測定された第2透過光の強度に基づき、前記計測対象液の前記第2測定波長における吸光度を算出し、該吸光度の値と、前記第2測定波長における油分の濃度と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める第2油分濃度決定部と
    を備えることを特徴とする請求項1に記載の洗浄液中の油分濃度計測装置。
    further,
    A second light irradiation unit that irradiates the measurement target liquid with a second irradiation light having a second measurement wavelength that is a predetermined one wavelength between 320 and 340 nm;
    A second transmitted light detector that measures the intensity of the second transmitted light through which the second irradiation light has passed through the measurement target liquid;
    Based on the intensity of the second transmitted light measured by the second transmitted light detection unit, the absorbance at the second measurement wavelength of the measurement target liquid is calculated, and the value of the absorbance and the oil content at the second measurement wavelength are calculated. The apparatus for measuring an oil concentration in a cleaning liquid according to claim 1, further comprising a second oil concentration determining unit that obtains the concentration of the oil in the measurement target liquid based on a calibration curve indicating a relationship between the concentration and the absorbance. .
  3.  280~300nmの間の所定の1波長である測定波長を有する照射光を計測対象液に照射し、
     前記照射光が前記計測対象液を透過した透過光の強度を測定し、
     前記透過光の強度に基づき、前記計測対象液の前記測定波長における吸光度を算出し、該吸光度の値と、前記測定波長における油分と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める
    ことを特徴とする、洗浄液中の油分濃度計測方法。
    Irradiate the measurement target liquid with irradiation light having a predetermined measurement wavelength of 280 to 300 nm,
    Measure the intensity of transmitted light through which the irradiation light has passed through the measurement target liquid,
    Based on the intensity of the transmitted light, the absorbance at the measurement wavelength of the measurement target liquid is calculated, and based on the absorbance value and a calibration curve indicating the relationship between the oil content and the absorbance at the measurement wavelength, A method for measuring the concentration of oil in a cleaning liquid, characterized in that the concentration of oil is determined.
  4.  前記計測対象液が、炭素原子の多重結合を有しない分子から成るものであることを特徴とする請求項3に記載の洗浄液中の油分濃度計測方法。 4. The method for measuring an oil concentration in a cleaning liquid according to claim 3, wherein the liquid to be measured is composed of molecules having no multiple bonds of carbon atoms.
  5.  さらに、
     320~340nmの間の所定の1波長である第2測定波長を有する第2照射光を前記計測対象液に照射し、
     前記第2照射光が前記計測対象液を透過した第2透過光の強度を測定し、
     前記第2透過光の強度に基づき、前記計測対象液の前記第2測定波長における吸光度を算出し、該吸光度の値と、前記第2測定波長における油分と吸光度の関係を示す検量線に基づいて前記計測対象液中の油分の濃度を求める
    ことを特徴とする請求項3又は4に記載の洗浄液中の油分濃度計測方法。
    further,
    Irradiating the measurement target liquid with second irradiation light having a second measurement wavelength which is a predetermined one wavelength between 320 and 340 nm;
    Measuring the intensity of the second transmitted light through which the second irradiation light has passed through the measurement target liquid;
    Based on the intensity of the second transmitted light, the absorbance at the second measurement wavelength of the measurement target liquid is calculated, and based on the absorbance value and a calibration curve indicating the relationship between the oil content and the absorbance at the second measurement wavelength. The oil concentration measurement method in the cleaning liquid according to claim 3 or 4, wherein the oil concentration in the measurement target liquid is obtained.
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JP7037206B2 (en) 2020-01-27 2022-03-16 アクトファイブ株式会社 Steam cleaning vacuum drying device

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